Pyrrolidine → N4-(4-chlorophenyl)6-pyrrolidin-1-yl-pyrimidine-4,5-diamine

HRID 1246802

反応式

HRID 1246802 の反応式
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)[C:3]=1[NH2:16].[NH:17]1[CH2:21][CH2:20][CH2:19][CH2:18]1>C([O-])(O)=O.[Na+]>[Cl:15][C:12]1[CH:13]=[CH:14][C:9]([NH:8][C:4]2[C:3]([NH2:16])=[C:2]([N:17]3[CH2:21][CH2:20][CH2:19][CH2:18]3)[N:7]=[CH:6][N:5]=2)=[CH:10][CH:11]=1

参加物

4

反応物 2

HCID 31268PyrrolidineHCID 167263116-Chloro-N4-(4-chlorophenyl)pyrimidine-4,5-diamine

生成物 1

HCID 21905785N4-(4-chlorophenyl)6-pyrrolidin-1-yl-pyrimidine-4,5-diamine

試薬・触媒・溶媒 1

HCID 516892Sodium Bicarbonate溶媒

反応条件

温度
100 °C

実験手順

6-Chloro-N4-(4-chlorophenyl)-pyrimidine-4,5-diamine I-(1A-1)a (114 mg, 0.45 mmol) and pyrrolidine (1 ml, excess) were combined and heated with stirring at 100° C. for 2 hours. The reaction mixture was diluted with saturated NaHCO3 solution and extracted with ethyl acetate. The organic layers were combined, dried (Na2SO4), filtered, and evaporated to dryness to yield the desired compound I-(17A-1)a (131 mg, quantitative) as an orange-brown solid: +ESI MS (M+1) 290.3; 1H NMR (500 MHz, CD3OD) δ 7.85 (s, 1H), 7.45 (d, J=8.8 Hz, 2H), 7.26 (d, J=8.8 Hz, 2H), 3.63 (m, 4H), 1.96 (m, 4H).

後処理

  1. temperatureheated
  2. extractionextracted with ethyl acetate
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. customevaporated to dryness

出典と根拠

ORDレコード
ord-71d7bad0cd694211a11f6ce4945b6b59
出典データセット
uspto-grants-2006_10
特許番号
US07129239B2

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